超高效液相色谱-串联质谱法同时测定罗非鱼养殖淡水中的9种喹诺酮类药物含量

目的建立超高效液相色谱-串联质谱联用法(ultraperformanceliquidchromatography-tandemmass spectrometry, UPLC-MS/MS)测定罗非鱼养殖淡水中9种喹诺酮类药物的分析方法。方法探究优化色谱条件、固相萃取柱条件、洗脱液比例和体积等对回收率产生影响的主要因素。样液制成0.1 mol/L Na2EDTA-Mcllvaine缓冲溶液后调节pH为4.0、采用聚合物固相萃取柱进行净化,吹干浓缩、溶解过滤后,经乙腈和乙酸铵-甲酸水溶液梯度洗脱、色谱柱Poroshell 120 EC-C18(50 mm×2.1 mm, 2.7μm)分离、超高效液相色谱-串联质谱仪测定, 8种化合物内标法定量, 1种化合物外标法定量。结果 9种目标物的检出限为0.02～0.2 ng/L,平均回收率为80.1%～110.3%,相对标准偏差(relative standard deviation, RSD)均小于10%。结论本方法经济、简便、稳定、准确性高,能满足实际罗非鱼养殖淡水中9种喹诺酮类药物含量测定的要求。

Simultaneous determination of 9 kinds of quinolones in tilapia cultured fresh water by ultra performance liquid chromatography-tandem mass spectrometry

Objective To establish a method for the determination of 9 kinds of quinolones in tilapia cultured fresh water by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The main factors influencing the recovery were optimized, such as chromatographic conditions, solid-phase extraction column conditions, eluent ratio and volume optimization. The sample liquid made from 0.1 mol/L Na2EDTA- Mcllvaine buffer solution, was purified by polymer solid phase extraction column after adjusting the pH to 4.0, blow dry enrichment dissolved after filtering, then the sample was separated on chromatography column Poroshell 120 EC-C18 (50 mm to 2.1 mm, 2.7 microns) after gradient elution with acetonitrile and ammonium acetate-formic acid aqueous solution, and determined by UPLC-MS/MS. Eight compounds were quantified by internal standard method and one compound was quantified by external standard method. Results The limits of detection of the 9 targets were 0.02?0.2 ng/L, the average recoveries were 80.1%?110.3%, and the relative standard deviations were less than 10%. Conclusion This method is economical, simple, stable and accurate, and can meet the requirements of the determination of 9 quinolones in tilapia cultured fresh water.